ZnO–SnO 2 composite oxides with various molar ratios of Sn:Zn have been synthesized at different calcination temperatures via a facile cetyltrimethylammonium bromide (CTAB)-assisted co-precipitation method with Zn(NO 3 ) 2 ·6H 2 O and SnCl 4 ·5H 2 O as starting materials. XRD, TEM, SEM and BET were employed to characterize the as-prepared samples. It has been found that amorphous intermediates appear between the evolutions of ZnO and SnO 2 crystals. The photocatalytic properties of the composite oxides were investigated using photocatalytic degradation of methyl orange as the probe reaction. The results show that the ZnO–SnO 2 composite oxide with a cube morphology exhibits the best photocatalytic activity, which was prepared with a molar ratio of Zn:Sn of 2:1 and calcination temperature of 700°C.